CN1587040A - Comprehensive utilizing method for by-product in organic silicon methyl monomer production process - Google Patents
Comprehensive utilizing method for by-product in organic silicon methyl monomer production process Download PDFInfo
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- CN1587040A CN1587040A CN 200410051507 CN200410051507A CN1587040A CN 1587040 A CN1587040 A CN 1587040A CN 200410051507 CN200410051507 CN 200410051507 CN 200410051507 A CN200410051507 A CN 200410051507A CN 1587040 A CN1587040 A CN 1587040A
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- 239000006227 byproduct Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000000178 monomer Substances 0.000 title claims description 17
- 239000010703 silicon Substances 0.000 title description 2
- 229910052710 silicon Inorganic materials 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000007789 gas Substances 0.000 claims abstract description 35
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000009835 boiling Methods 0.000 claims description 24
- 229960001866 silicon dioxide Drugs 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000005543 nano-size silicon particle Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- 238000009834 vaporization Methods 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 4
- 229910008045 Si-Si Inorganic materials 0.000 claims description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 3
- 229910002808 Si–O–Si Inorganic materials 0.000 claims description 3
- 229910006411 Si—Si Inorganic materials 0.000 claims description 3
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 3
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 13
- 229920001971 elastomer Polymers 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000005060 rubber Substances 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract 3
- 229910052682 stishovite Inorganic materials 0.000 abstract 3
- 229910052905 tridymite Inorganic materials 0.000 abstract 3
- 238000005345 coagulation Methods 0.000 abstract 1
- 230000015271 coagulation Effects 0.000 abstract 1
- 238000012643 polycondensation polymerization Methods 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 12
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 6
- 239000005049 silicon tetrachloride Substances 0.000 description 6
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000005055 methyl trichlorosilane Substances 0.000 description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 2
- 150000001282 organosilanes Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- XLVKXZZJSTWDJY-UHFFFAOYSA-N [SiH4].[Si] Chemical compound [SiH4].[Si] XLVKXZZJSTWDJY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007233 catalytic pyrolysis Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 150000001367 organochlorosilanes Chemical class 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The comprehensive utilizing process of the by product includes gasifying the by product, pre-mixing the gas with hydrogen and air, feeding gas mixture to burning nozzle continuously, high temperature hydrolysis and condensation polymerization in flame of 1000-2000 deg.c in reaction chamber, coagulation, cyclonic gas-solid separation, and deacidification to obtain nanometer SiO2. The nanometer SiO2 product thus prepared has particle size of 7-40 nm, specific surface area of 100-400 sq m/g, pH 3.8-4.5 and SiO2 content greater than 99.8 %, and may be used widely in organosilicon, rubber, plastic, paint, electronics and other fields for reinforcing, densifying, thixotropy, etc.
Description
Technical field
The present invention relates to the method for comprehensive utilization of the by product that produces in a kind of organosilicon methyl monomer production process.
Background technology
Organic halosilanes particularly methyl chlorosilane is preparation organosilicon polymer (silicone oil, silicon rubber and silicone resin) and other functionalized silicon silane most important material, wherein again with the consumption maximum of dimethyldichlorosilane(DMCS) (account for methyl chlorosilane 90%).Therefore the synthetic method that obtains the dimethyldichlorosilane(DMCS) of high yield becomes the key of organosilicon methyl monomer industrial development.
Nineteen forty-one E.G.Rochow has at first proposed the synthetic organochlorosilane of direct method, and it is under heating and copper catalyst effect, produce halosilanes by halohydrocarbon and elemental silicon direct reaction, thereby this method is called direct method.Be characterized in that raw material is easy to get, operation is simple, without solvent, productive rate height, and be easy to realize advantage such as continuous mass production.This method has just replaced traditional method once coming out, and becomes the unique method of industrial production methyl chlorosilane.In the industrial production in the direct method synthetic product yield of dimethyldichlorosilane(DMCS) be 75～85%, also has 15～25% by product, the boiling point of dimethyldichlorosilane(DMCS) is 70.2 ℃, therefore the cut that is lower than 70.2 ℃ is called low-boiling-point substance, account for 10～15%, and be higher than 70.2 ℃ cut for high boiling material, account for 5～10%.Table 1 is the main composition of direct method synthetic product.
Silicone monomer industry in China developed rapidly in recent years, and monomer throughput improves very fast, and table 2 is the industrial scale of the main organosilane monomer manufacturing enterprise of China and capability forecasting in 2006.Owing to contain hydrolyzable chlorine atom in the by product, and their boiling points are not high, discharging or placement all can produce acid attack, pollute.Therefore the outlet of organosilicon by product has become the bottleneck problem of constraint organosilicon methyl monomer industrial development.
Research about the comprehensive utilization of organosilicon by product is also very many, and traditional method has the METHYL TRICHLORO SILANE in the low-boiling-point substance (accounting for low-boiling-point substance more than 50%) is used to prepare waterproof paint, silicone resin and branched chain type silicone oil.And in comprehensive utilization of high boiling, mainly contain and utilize the high boiling material hydrolysis to prepare waterproofing agent of organosilicon, can utilize high boiling material to prepare silicone oil, silicone resin, defoamer and remover etc. in addition, U.S. Pat 5907050 is to adopt the high boiling material catalytic pyrolysis is produced methyl chlorosilane, U.S. Pat 5922893 is that silicomethane is produced in by product cracking, hydrogenation, but generally only has the high boiling material ability of two chlorine atoms on a Siliciumatom at least
Table 1 methyl chlorosilane product is formed
| The component title | Molecular formula | Boiling point (101.3kPa)/℃ | ||
| Principal product | Dimethyldichlorosilane(DMCS) | (CH 3) 2SiCl 2 | ???70.2 | |
| By product | Low-boiling-point substance | METHYL TRICHLORO SILANE | CH 3SiCl 3 | ???66.1 |
| Trimethylchlorosilane | (CH 3) 3SiCl | ???57.3 | ||
| Dimethyl dichlorosilane (DMCS) | CH 3SiHCl 2 | ???40.4 | ||
| Dimethylchlorosilane | (CH 3) 2SiHCl | ???35.4 | ||
| Tetramethylsilane | (CH 3) 4Si | ???26.2 | ||
| Silicon tetrachloride | SiCl 4 | ???57.6 | ||
| Trichlorosilane | HSiCl 3 | ???31.8 | ||
| High boiling material | Disilane etc. | ≡Si-Si≡ ≡Si-O-Si≡ ≡Si-CH 2-Si≡ | ???＞70.2℃ | |
Industrial scale unit of the domestic main organosilane monomer of table 2 manufacturing enterprise: ten thousand tons
Manufacturing enterprise 2000 2002 2006
Blue star spark chemical plant 1.5 7.0 20.0
New Anhua worker 1.5 3.5 8.0
Jilin chemical industry 1.8 2.5 12.5
Beijing chemical industry two factories 0.5 0.5--
Aggregated capacity 5.3 13.5 40.5
By product 1.0 2.0 5.0
Enough cracking, therefore this method can not make full use of high boiling material, and also more complicated of these methods.Though traditional method can be fully utilized high-boiling and low-boiling components, they all are very limited to the digestion amount of by product, and also there are difficulties such as separation in some, can not utilize fully.Along with the raising of silicone monomer industry production level and output, it is extremely important that the comprehensive utilization of by product will become, and can promote the development of silicone monomer industry greatly.
Summary of the invention
The object of the present invention is to provide the comprehensive use of the by product in a kind of organosilicon methyl monomer production process, the characteristics of this method are to make full use of by product, the nano silicon of production high added value, and be easy to suitability for industrialized production.
The comprehensive use of the by product in a kind of organosilicon methyl monomer production process provided by the invention, this method is with by product vaporization back and hydrogen, air pre-mixing, be transported to burner noz(zle) then continuously, in reaction chamber, in 1000～2000 ℃ flame, carry out the pyrohydrolysis polycondensation, separate and the depickling aftertreatment technology through overbunching, cyclone gas-solid again, make the nano silicon of high added value at last.
By product of the present invention is meant high boiling material or the low-boiling-point substance that is produced in the organosilicon methyl monomer production process, and wherein high boiling material is meant and mainly contains ≡ Si-Si ≡, ≡ Si-O-Si ≡ and ≡ Si-CH
2The mixture of disilane such as-Si ≡, low-boiling-point substance is meant and mainly contains SiCl
4, HSiCl
3,, (CH
3)
4Si,, (CH
3)
2SiHCl,, CH
3SiHCl
2,, (CH
3)
3The mixture of silicomethanes such as SiCl.
Burner noz(zle) of the present invention is positioned at the top of reaction chamber, has certain distance between burner noz(zle) and the reaction chamber, and burner noz(zle) is provided with a chuck, has the inlet of a conveying hydrogen on the chuck.
Cyclone gas-solid separating technology of the present invention adopts three cyclonic separators to separate, the silicon-dioxide of flash trapping stage directly enters the depickling stove, tail gas enters secondary to be separated, secondary separates the tail gas that produces and enters three grades of separation, two, three grades of isolating silicon-dioxide return flash trapping stage, and three grades of isolating tail gas enter exhaust treatment system.
Deacidifying process of the present invention adopts depickling stove high-temperature calcination depickling, heating tube by cross arrangement in the depickling stove heats, make the interior temperature of depickling stove remain on 400～700 ℃, simultaneously in the depickling stove, feed assist gas, the ingress that assist gas enters the depickling stove is provided with a well heater, well heater heats assist gas, the temperature that makes assist gas before entering the depickling stove between 160～260 ℃.
The present invention is the mixed gas of nitrogen or nitrogen and water vapour at the assist gas described in the deacidifying process.
Compare with the treatment process of by product in the traditional organosilicon methyl monomer production process, characteristics of the present invention are to make full use of by product, and its primary particle diameter of the nano silicon of preparation is 7～40nm, and specific surface area is at 100～400m
2Between/the g, pH value is 3.8～4.5, and dioxide-containing silica is greater than 99.8%, and product can be widely used in fields such as organosilicon, rubber, plastics, coating, electronics, plays functions such as reinforcement, thickening, thixotroping, anti-sedimentation.
The present invention is further illustrated below in conjunction with the drawings and the specific embodiments.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the structural representation of burner noz(zle) of the present invention and reaction chamber.
Embodiment
In concrete enforcement, if adopt the organosilicon by product fully, because reaction heat is than higher during burning, the claimed apparatus cooling efficiency is very high, therefore actual general organosilicon by product and the silicon tetrachloride use that is mixed of adopting, the technology controlling and process ratio is easier to, the also relatively good control of the quality of product, and the silicon tetrachloride consumption generally accounts for 10～80% of mixture.
With the mixture of the high boiling material in the by product or low-boiling-point substance and silicon tetrachloride through overflash, carry out premix with hydrogen and air, as shown in Figure 1, the high boiling material that mixes of process premix or low-boiling-point substance, hydrogen, oxygen enter burner noz(zle) 1 continuously, combustion reactions in reaction chamber 2, the water that high boiling material or low-boiling-point substance utilization burning generate and the heat of generation carry out the pyrohydrolysis condensation reaction, and generating particle diameter is the aerosil of 7～40 nanometers.Aerosil enters collector 3, through the silica aggregate of about 1 micron of formation behind the overbunching.Silica aggregate and reactor off-gas enter primary cyclone 4 together then, silica aggregate is separated with reactor off-gas, silicon-dioxide flows downward, enter depickling stove 7, reactor off-gas and part silicon-dioxide then upwards flow, enter secondary cyclone 5 and carry out the secondary separation, the isolating tail gas of secondary enters three grades of separators 6, two, three grades of silicon-dioxide that separate gained return flash trapping stage, three grades of isolating tail gas enter exhaust treatment system, can guarantee that like this yield of silicon-dioxide is greater than 99%.
Also be adsorbed with many HCl gases in the silicon-dioxide after the separation, make that the pH value of product is too low, limited the application of product, thereby must handle, remove the HCl of silica sphere absorption through depickling.The present invention adopts the method for high-temperature calcination depickling, as shown in Figure 1, silicon-dioxide after primary cyclone 4 separates directly enters the depickling stove 7, and the bottom from depickling stove 7 feeds the depickling assist gas simultaneously, and assist gas can be the mixed gas of nitrogen or nitrogen and water vapour.Enter the ingress of depickling stove 7 at assist gas, have 8 pairs of assist gass of a well heater to heat, guarantee that assist gas enters that temperature is between 160～260 ℃ before the depickling stove 7, first-selected 210～230 ℃.In depickling stove 7,, guarantee that temperature is between 400～700 ℃, between first-selected 500～600 ℃ in the stove by staggered heating tube heating.By silicon-dioxide is carried out high-temperature calcination, make HCl from the absorption of silicon dioxide meter emaciated face, take away by assist gas.The silicon-dioxide that comes out from depickling stove 7 enters basin 9, and tail gas then enters exhaust treatment system, and through after the depickling, the pH value of 4% aqeous suspension of product can satisfy the service requirements in most of fields greater than 3.8.
Reaction mixture gas body auto-combustion nozzle 1 enters reaction chamber 2 among the present invention, burner noz(zle) 1 is provided with a chuck 10, from the inlet 14 of the conveying hydrogen of chuck 10, feed hydrogen, can around nozzle, form uniform annular space oxyhydrogen flame 12, oxyhydrogen flame flows along reaction chamber 2 inwalls, surrounds reaction flame 11, has reduced the silicon dioxide granule of reaction generation and contacting of reaction chamber 2 inwalls, above preventing that it is deposited on, guarantee normally carrying out of pyrohydrolysis condensation reaction simultaneously.Leave certain distance between burner noz(zle) 1 and the reaction chamber 2, be convenient to light annular space flame 12, supplements cold 13 in roasting kiln reduces furnace temperature simultaneously, prolongs the work-ing life of roasting kiln.In the traditional technology, nozzle interior must keep malleation preventing tempering, and adopts burner noz(zle) 1 of the present invention, owing in chuck 10, feed hydrogen, even burner noz(zle) 1 internal pressure is zero or little negative pressure, also can prevent burner noz(zle) generation tempering, improved the security of producing.Burner noz(zle) 1 and reaction chamber 2 that the present invention adopts, can avoid the deposition of nano silicon on reaction chamber wall in the production process, improve the cooling performance of roasting kiln, effectively prolonged the work-ing life of roasting kiln, thereby guaranteed the continuity of production and the stability of product.
Embodiment 1: organosilicon high-boiling product and silicon tetrachloride mixture (weight ratio 3: 7) (boiling range is 100～140 ℃), 140～150 ℃ of vaporizations down, mix with hydrogen, air (preheating temperature is 120～140 ℃) after the preheating then, wherein organosilicon high-boiling product is pressed 70Kg/h, 7 cubic metres/h of hydrogen, the supply of 220 cubic metres/h of air ratio, mixed gas delivers into the roasting kiln nozzle continuously, react by above-mentioned embodiment, temperature is 540 ℃ in the depickling stove, the temperature of water vapor and nitrogen is 210 ℃, prepared silicon-dioxide quality index:
Dioxide-containing silica (%) 99.80
The primary partical averageparticle is (nm) 18 all
Specific surface area (m
2/ g) 160
PH value (4% suspension) 3.98
Carbon content (%) 0.01
Embodiment 2: organosilicon low-boiling-point substance and silicon tetrachloride (weight ratio 6: 4) (35～67 ℃ of boiling ranges) are 80～90 ℃ of vaporizations down, press low-boiling-point substance 65Kg/h then, hydrogen is with 7.5 cubic metres/h, the mixed of 200 cubic metres/h of air (hydrogen and air are 120～140 ℃ of preheatings), other processing parameter is identical with embodiment 1.The silicon-dioxide quality index that makes:
Dioxide-containing silica (%) 99.78
Primary partical median size (nm) 16
Specific surface area (m2/g) 156
PH value (4% suspension) 3.88
Carbon content (%) 0.01
Claims (7)
1, the comprehensive use of the by product in a kind of organosilicon methyl monomer production process, it is characterized in that: with by product vaporization back and hydrogen, air pre-mixing, be transported to burner noz(zle) then continuously, in reaction chamber, in 1000～2000 ℃ flame, carry out the pyrohydrolysis polycondensation, separate and the depickling aftertreatment technology through overbunching, cyclone gas-solid again, make the nano silicon of high added value at last.
2, the described comprehensive use of root a tree name claim 1 is characterized in that: described by product is meant high boiling material or the low-boiling-point substance that is produced in the organosilicon methyl monomer production process.
3, comprehensive use according to claim 2 is characterized in that: described high boiling material is meant and mainly contains ≡ Si-Si ≡, ≡ Si-O-Si ≡ and ≡ Si-CH
2The mixture of the disilane of-Si ≡ class, low-boiling-point substance are meant and mainly contain SiCl
4, HSiCl
3,, (CH
3)
4Si,, (CH
3)
2SiHCl,, CH
3SiHCl
2,, (CH
3)
3The mixture of the silicomethane of SiCl class.
4, comprehensive use according to claim 1, it is characterized in that: described burner noz(zle) is positioned at the top of reaction chamber, have certain distance between burner noz(zle) and the reaction chamber, burner noz(zle) is provided with a chuck, has the inlet of a conveying hydrogen on the chuck.
5, comprehensive use according to claim 1, it is characterized in that: described cyclone gas-solid separating technology adopts three cyclonic separators to separate, the silicon-dioxide of flash trapping stage directly enters the depickling stove, tail gas enters secondary to be separated, secondary separates the tail gas that produces and enters three grades of separation, two, three grades of isolating silicon-dioxide return flash trapping stage, and three grades of isolating tail gas enter exhaust treatment system.
6, comprehensive use according to claim 1, it is characterized in that: described deacidifying process adopts depickling stove high-temperature calcination depickling, heating tube by cross arrangement in the depickling stove heats, make the interior temperature of depickling stove remain on 400～700 ℃, simultaneously in the depickling stove, feed assist gas, the ingress that assist gas enters the depickling stove is provided with a well heater, and well heater heats assist gas, the temperature that makes assist gas before entering the depickling stove between 160～260 ℃.
7, comprehensive use according to claim 6 is characterized in that: described assist gas is the mixed gas of nitrogen or nitrogen and water vapour.
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|---|---|---|---|
| CN 200410051507 CN1238252C (en) | 2004-09-17 | 2004-09-17 | Comprehensive utilizing method for by-product in organic silicon methyl monomer production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410051507 CN1238252C (en) | 2004-09-17 | 2004-09-17 | Comprehensive utilizing method for by-product in organic silicon methyl monomer production process |
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|---|---|
| CN1587040A true CN1587040A (en) | 2005-03-02 |
| CN1238252C CN1238252C (en) | 2006-01-25 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100369811C (en) * | 2006-04-29 | 2008-02-20 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN101378991B (en) * | 2006-03-03 | 2012-11-28 | 瓦克化学有限公司 | Process for recycling high-boiling compounds within an integrated chlorosilane system |
| CN107603230A (en) * | 2017-08-25 | 2018-01-19 | 山东东岳有机硅材料有限公司 | Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof |
| CN109880119A (en) * | 2019-01-31 | 2019-06-14 | 山东东岳有机硅材料股份有限公司 | Elimination organosilicon crude monomer hydrolysate is not stratified and sticks the method for equipment phenomenon |
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| CN102513031B (en) * | 2011-11-30 | 2014-04-16 | 广州吉必盛科技实业有限公司 | Deacidification process and equipment thereof |
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| CN101378991B (en) * | 2006-03-03 | 2012-11-28 | 瓦克化学有限公司 | Process for recycling high-boiling compounds within an integrated chlorosilane system |
| CN100369811C (en) * | 2006-04-29 | 2008-02-20 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN107603230A (en) * | 2017-08-25 | 2018-01-19 | 山东东岳有机硅材料有限公司 | Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof |
| CN109880119A (en) * | 2019-01-31 | 2019-06-14 | 山东东岳有机硅材料股份有限公司 | Elimination organosilicon crude monomer hydrolysate is not stratified and sticks the method for equipment phenomenon |
| CN109880119B (en) * | 2019-01-31 | 2021-08-10 | 山东东岳有机硅材料股份有限公司 | Method for eliminating phenomena of no delamination and equipment adhesion of organosilicon crude monomer hydrolysate |
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| CN114015049A (en) * | 2021-10-29 | 2022-02-08 | 山东东岳有机硅材料股份有限公司 | Preparation method of MQ silicon resin for synthesizing pressure-sensitive adhesive from organic silicon by-product |
| CN114015049B (en) * | 2021-10-29 | 2023-10-24 | 山东东岳有机硅材料股份有限公司 | Preparation method of MQ silicon resin for synthesizing pressure-sensitive adhesive from organic silicon byproducts |
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